EP2994707B1 - Verfahren zur erzeugung von salzen mit reduziertem kristallwassergehalt - Google Patents

Verfahren zur erzeugung von salzen mit reduziertem kristallwassergehalt Download PDF

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Publication number
EP2994707B1
EP2994707B1 EP14726514.4A EP14726514A EP2994707B1 EP 2994707 B1 EP2994707 B1 EP 2994707B1 EP 14726514 A EP14726514 A EP 14726514A EP 2994707 B1 EP2994707 B1 EP 2994707B1
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EP
European Patent Office
Prior art keywords
drying
water
gas
moisture content
dryer
Prior art date
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Active
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EP14726514.4A
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German (de)
English (en)
French (fr)
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EP2994707A1 (de
Inventor
Paul Bernhard Kröhl
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Andritz Technology and Asset Management GmbH
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Andritz Technology and Asset Management GmbH
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Priority to SI201430664T priority Critical patent/SI2994707T1/en
Priority to PL14726514T priority patent/PL2994707T3/pl
Publication of EP2994707A1 publication Critical patent/EP2994707A1/de
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    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F26—DRYING
    • F26B—DRYING SOLID MATERIALS OR OBJECTS BY REMOVING LIQUID THEREFROM
    • F26B21/00—Arrangements or duct systems, e.g. in combination with pallet boxes, for supplying and controlling air or gases for drying solid materials or objects
    • F26B21/06—Controlling, e.g. regulating, parameters of gas supply
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
    • C01D5/00—Sulfates or sulfites of sodium, potassium or alkali metals in general
    • C01D5/18—Dehydration
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F26—DRYING
    • F26B—DRYING SOLID MATERIALS OR OBJECTS BY REMOVING LIQUID THEREFROM
    • F26B3/00—Drying solid materials or objects by processes involving the application of heat
    • F26B3/02—Drying solid materials or objects by processes involving the application of heat by convection, i.e. heat being conveyed from a heat source to the materials or objects to be dried by a gas or vapour, e.g. air
    • F26B3/04—Drying solid materials or objects by processes involving the application of heat by convection, i.e. heat being conveyed from a heat source to the materials or objects to be dried by a gas or vapour, e.g. air the gas or vapour circulating over or surrounding the materials or objects to be dried
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
    • C01D1/00—Oxides or hydroxides of sodium, potassium or alkali metals in general
    • C01D1/04—Hydroxides
    • C01D1/44—Preparation in the form of granules, pieces, or other shaped products
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
    • C01D3/00—Halides of sodium, potassium or alkali metals in general
    • C01D3/22—Preparation in the form of granules, pieces, or other shaped products
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
    • C01D7/00—Carbonates of sodium, potassium or alkali metals in general
    • C01D7/35—Varying the content of water of crystallisation or the specific gravity
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
    • C01D9/00—Nitrates of sodium, potassium or alkali metals in general
    • C01D9/18—Preparation in the form of shaped products, e.g. granules
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
    • C01F11/00—Compounds of calcium, strontium, or barium
    • C01F11/20—Halides
    • C01F11/24—Chlorides
    • C01F11/30—Concentrating; Dehydrating; Preventing the adsorption of moisture or caking
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
    • C01F5/00—Compounds of magnesium
    • C01F5/26—Magnesium halides
    • C01F5/30—Chlorides
    • C01F5/34—Dehydrating magnesium chloride containing water of crystallisation
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
    • C01F7/00—Compounds of aluminium
    • C01F7/48—Halides, with or without other cations besides aluminium
    • C01F7/56—Chlorides
    • C01F7/58—Preparation of anhydrous aluminium chloride
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G49/00—Compounds of iron
    • C01G49/14—Sulfates
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F26—DRYING
    • F26B—DRYING SOLID MATERIALS OR OBJECTS BY REMOVING LIQUID THEREFROM
    • F26B17/00—Machines or apparatus for drying materials in loose, plastic, or fluidised form, e.g. granules, staple fibres, with progressive movement
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F26—DRYING
    • F26B—DRYING SOLID MATERIALS OR OBJECTS BY REMOVING LIQUID THEREFROM
    • F26B21/00—Arrangements or duct systems, e.g. in combination with pallet boxes, for supplying and controlling air or gases for drying solid materials or objects
    • F26B21/02—Circulating air or gases in closed cycles, e.g. wholly within the drying enclosure
    • F26B21/04—Circulating air or gases in closed cycles, e.g. wholly within the drying enclosure partly outside the drying enclosure
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F26—DRYING
    • F26B—DRYING SOLID MATERIALS OR OBJECTS BY REMOVING LIQUID THEREFROM
    • F26B21/00—Arrangements or duct systems, e.g. in combination with pallet boxes, for supplying and controlling air or gases for drying solid materials or objects
    • F26B21/06—Controlling, e.g. regulating, parameters of gas supply
    • F26B21/08—Humidity
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F26—DRYING
    • F26B—DRYING SOLID MATERIALS OR OBJECTS BY REMOVING LIQUID THEREFROM
    • F26B21/00—Arrangements or duct systems, e.g. in combination with pallet boxes, for supplying and controlling air or gases for drying solid materials or objects
    • F26B21/06—Controlling, e.g. regulating, parameters of gas supply
    • F26B21/08—Humidity
    • F26B21/086—Humidity by condensing the moisture in the drying medium, which may be recycled, e.g. using a heat pump cycle
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F26—DRYING
    • F26B—DRYING SOLID MATERIALS OR OBJECTS BY REMOVING LIQUID THEREFROM
    • F26B3/00—Drying solid materials or objects by processes involving the application of heat
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F26—DRYING
    • F26B—DRYING SOLID MATERIALS OR OBJECTS BY REMOVING LIQUID THEREFROM
    • F26B3/00—Drying solid materials or objects by processes involving the application of heat
    • F26B3/02—Drying solid materials or objects by processes involving the application of heat by convection, i.e. heat being conveyed from a heat source to the materials or objects to be dried by a gas or vapour, e.g. air
    • F26B3/06—Drying solid materials or objects by processes involving the application of heat by convection, i.e. heat being conveyed from a heat source to the materials or objects to be dried by a gas or vapour, e.g. air the gas or vapour flowing through the materials or objects to be dried
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F26—DRYING
    • F26B—DRYING SOLID MATERIALS OR OBJECTS BY REMOVING LIQUID THEREFROM
    • F26B3/00—Drying solid materials or objects by processes involving the application of heat
    • F26B3/18—Drying solid materials or objects by processes involving the application of heat by conduction, i.e. the heat is conveyed from the heat source, e.g. gas flame, to the materials or objects to be dried by direct contact
    • F26B3/20—Drying solid materials or objects by processes involving the application of heat by conduction, i.e. the heat is conveyed from the heat source, e.g. gas flame, to the materials or objects to be dried by direct contact the heat source being a heated surface, e.g. a moving belt or conveyor
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00—Physical properties of inorganic compounds
    • C01P2006/80—Compositional purity
    • C01P2006/82—Compositional purity water content
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F26—DRYING
    • F26B—DRYING SOLID MATERIALS OR OBJECTS BY REMOVING LIQUID THEREFROM
    • F26B2200/00—Drying processes and machines for solid materials characterised by the specific requirements of the drying good

Definitions

  • the invention relates to a process for drying salts containing water of crystallization in convective apparatus.
  • High water content products such as Glauber's salt (magnesium sulfate * 10 water)
  • Glauber's salt magnesium sulfate * 10 water
  • abrasion-sensitive, dusty and fine-grained products are obtained or stable and low-dust granules or intermediate stages transition stages of the two qualities. Drying typically takes place in rotary dryers (drum dryers), tubular dryers or fluidized bed dryers with or without built-in heat exchangers. Also, spray granulation in the fluidized bed is used, but is less economical because of the higher water evaporation. In part, the drying processes are also combined.
  • Such methods for drying of salts containing water of crystallization are, for example, from GB 805159 known, which generally describes a drying.
  • the DE 1113666 describes a dust recycling and the GB 388553 describes a drying by means of vacuum.
  • the aim of the invention is therefore the production of salts with reduced crystal water content with certain properties, regardless of the method used, the properties depend essentially on the bulk density.
  • the invention is therefore characterized in that the drying above a specified moisture content, for example above an absolute humidity of 10%, of the drying gas, wherein the moisture content of the drying gas is set above the set moisture value by complete recycling of the same, the evaporated water from the Cycle is removed by condensation and the moisture content of the drying gas is adjusted by means of the condenser temperature.
  • the gas that surrounds the salt particles during drying thus has a certain humidity. This influences the drying speed.
  • the water initially evaporates spontaneously at the surface, as a result of the then increasing temperature, further water of crystallization is released inside the particle, evaporated and passed through pores and capillaries to the surface.
  • the capillaries and pores are widened, creating a porous particle with a low density and a weakened structure.
  • the partially formed salt solution can partially close or reduce pores, cracks and capillaries again. This results in a solid particle of high density.
  • salts with high levels of water of crystallization eg decahydrates such as Glauber's salt (sodium sulfate) give off water of crystallization even at low temperatures (well below 100 °). Because of the low temperatures, it does not evaporate sufficiently and the salt melts or bakes.
  • a favorable development of the invention is therefore characterized in that dust and / or dried product is combined with the moist salt containing water of crystallization before drying and optionally mixed.
  • the excess free water of crystallization can be bound by recombination and gives an uncritical mixture, which can be dried further.
  • This back-mixing is typically carried out in a mixer upstream of the dryer, but can also be carried out in the dryer by appropriate design of the dryer geometry.
  • An advantageous development of the invention is characterized in that in place of dust and / or in addition to dust ground oversize is combined with the moist salt containing water of crystallization ("dusting").
  • a favorable development of the invention is characterized in that the moisture content only in a geometrical portion of the dryer, e.g. in the task zone, is set.
  • the gas continues the vaporized water
  • the energy supply can also be made by the gas and / or by contact surfaces.
  • the exhaust gas humidity is usually too low, so the hot gas temperature and flow rate with the help of the energy balance to be chosen so that the water vaporized thereby raises the exhaust gas moisture in the desired range.
  • This does not necessarily succeed in all types of salt and dryer.
  • convective appliances with indirect heating can set the water evaporation rate, on the one hand, via the temperature of the heating surfaces and on the other others about the size of the same.
  • the vaporized water is condensed in a condenser and discharged from the circulation.
  • the temperature of the condenser determines the exhaust gas humidity.
  • Exemplary Embodiment 1 In a fluidized-bed dryer with a built-in heat exchanger in the layer, surface-moist iron sulfate heptahydrate was dried to monohydrate. 420 kg / h of moist heptahydrate and 260 kg / h of dry residue (monohydrate product and dust from drying) were fed to the dryer via a mixer. The drying air (1300kg / h) had a temperature of 185 ° C, the heat exchanger of 195 ° and the product layer of 117 ° C. Together with the initial load of 10g / kg of dry air, the vaporized water produced an exhaust load of 146g / kg tr. L.
  • Exemplary Embodiment 2 In the same dryer, the same amount of heptahydrate and backbone consisting of monohydrate and dust was dried from drying at almost the same temperatures (air 178 °, heat exchanger 195 °, product layer 120 °). The main difference to Example 1 was that the air was completely returned and the evaporated water was condensed out in a scrubber. Because of the changing Product had to be raised the Kreisluft concept to 1730 kg / h. The scrubber had a temperature of 65 °, resulting in a total loading of 205g water / kg tr.L. the air fed back to the dryer.
  • the exhaust air after the dryer then had a loading of 329 g / kg, which corresponds to an absolute humidity of 24.8% and a dew point of about 73 °.
  • a stable and heavy monohydrate was produced with a bulk density of 1195 g / l, a mean grain diameter of 450 microns and a dust discharge with the exhaust air of only 15%.
  • the supply air fan 10 presses ambient air through a heater 11 in the drying apparatus (here a fluidized bed dryer) 12, in which the salt is optionally heated by the heat exchanger 13 and emits the water of crystallization.
  • the moist drying gas leaves the dryer, is freed from dust in a filter or cyclone 14 and passes for an optional additional gas cleaning through the exhaust fan 18 into the open 19.
  • the surface moisture, crystal water-containing salt 20 is in the mixer 21 with the separated dust from cyclone or filter 14 and optionally powdered with recycled product and fed to the dryer 12. After drying, it leaves the dryer 12 and in an optional sieve 22 oversize is separated, ground 23 and fed to the mixer 21.
  • the good fraction passes into an overflow silo 24, from which optionally return material for the mixer 21 is withdrawn by means of a metering screw 25 and the end product 26 passes to further processing.
  • Fig. 2 is the variant of the drying process with partial gas recirculation for setting a defined gas humidity, ie a specified moisture content in the dryer shown.
  • the product treatment is the same as in Fig. 1 described and not shown for clarity.
  • the fan 10 presses the gas in the circuit through the heating coil 11, dryer 12 and dust collector 14.
  • a partial flow of fresh air is metered in via the optional filter 15.
  • the corresponding amount of moist exhaust gas is discharged via the pressure-controlled throttle member 17 on the pressure side of the fan.
  • This exhaust stream 19 also contains the vaporized amount of water of the product. The smaller the fresh air partial flow, the higher the gas humidity.
  • the evaporated water must be selectively removed from the recycle gas. This is conveniently done by condensation in a surface or a wash condenser 30.
  • the wash water is pumped in a circle 31 and the heat of condensation is removed via the cooler 32.
  • the condensed amount of water, which also corresponds to the evaporated amount of water from the product is level controlled 33 removed from the process.
  • the temperature of the wash water can be adjusted so that the required initial moisture content of the cycle gas results from the partial vapor pressure of the water.
  • the initial moisture content is calculated from the desired exhaust gas moisture content minus the proportion produced by the evaporation of water from the product.
  • the circulating gas is circulated by the blower 10 via heating register 11, dryer 12, dust collector 14 and washing capacitor 30.
  • the product path here corresponds to the Fig.1 and is not shown for clarity again.
  • the systems shown are only exemplary and illustrated by the example of a fluidized bed dryer (with or without built-in heat exchanger). However, it is also possible to use rotary tube dryers (drum dryers), tubular dryers or fluidized bed spray granulators.

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  • Engineering & Computer Science (AREA)
  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • General Engineering & Computer Science (AREA)
  • Mechanical Engineering (AREA)
  • Inorganic Chemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Materials Engineering (AREA)
  • Microbiology (AREA)
  • Geology (AREA)
  • Agronomy & Crop Science (AREA)
  • Drying Of Solid Materials (AREA)
  • Vaporization, Distillation, Condensation, Sublimation, And Cold Traps (AREA)
  • Processing And Handling Of Plastics And Other Materials For Molding In General (AREA)
  • Medicines Containing Material From Animals Or Micro-Organisms (AREA)
EP14726514.4A 2013-05-07 2014-05-02 Verfahren zur erzeugung von salzen mit reduziertem kristallwassergehalt Active EP2994707B1 (de)

Priority Applications (2)

Application Number Priority Date Filing Date Title
SI201430664T SI2994707T1 (en) 2013-05-07 2014-05-02 A process for the production of salt with a reduced crystal water content
PL14726514T PL2994707T3 (pl) 2013-05-07 2014-05-02 Sposób wytwarzania soli o zredukowanej zawartości wody krystalizacyjnej

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
ATA379/2013A AT514275B1 (de) 2013-05-07 2013-05-07 Verfahren zur Erzeugung von Salzen mit reduziertem Kristallwassergehalt
PCT/EP2014/001177 WO2014180547A1 (de) 2013-05-07 2014-05-02 Verfahren zur erzeugung von salzen mit reduziertem kristallwassergehalt

Publications (2)

Publication Number Publication Date
EP2994707A1 EP2994707A1 (de) 2016-03-16
EP2994707B1 true EP2994707B1 (de) 2018-01-10

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EP14726514.4A Active EP2994707B1 (de) 2013-05-07 2014-05-02 Verfahren zur erzeugung von salzen mit reduziertem kristallwassergehalt

Country Status (18)

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US (2) US10215492B2 (ja)
EP (1) EP2994707B1 (ja)
JP (1) JP6383784B2 (ja)
KR (1) KR102131821B1 (ja)
CN (1) CN105190211B (ja)
AT (1) AT514275B1 (ja)
AU (1) AU2014264996B2 (ja)
BR (1) BR112015027191B1 (ja)
CA (1) CA2910678C (ja)
ES (1) ES2665143T3 (ja)
MX (1) MX366370B (ja)
MY (1) MY175972A (ja)
PL (1) PL2994707T3 (ja)
RU (1) RU2655442C2 (ja)
SG (1) SG11201508937TA (ja)
SI (1) SI2994707T1 (ja)
UA (1) UA118675C2 (ja)
WO (1) WO2014180547A1 (ja)

Families Citing this family (5)

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US11221180B2 (en) * 2019-04-02 2022-01-11 Innovative Environmental Companies, Inc. Systems and methods related to staged drying of temperature sensitive materials
CN111609673A (zh) * 2020-06-02 2020-09-01 湖南省湘衡盐化有限责任公司 一种工业盐干燥设备及其方法
DE102021125452B4 (de) 2021-09-30 2024-06-27 Dr. Weigel Anlagenbau Gmbh Trocknungsvorrichtung und Verfahren zum Betreiben einer Trocknungsvorrichtung
AU2022268395B2 (en) * 2022-03-16 2023-12-14 Gea Process Engineering A/S Method and system for drying salts, in particular hydrated salt
AR128797A1 (es) 2022-03-16 2024-06-12 Gea Process Eng A/S Método y sistema para secar sales, en particular sales hidratadas

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RU2015150297A (ru) 2017-06-08
RU2655442C2 (ru) 2018-05-28
KR102131821B1 (ko) 2020-07-09
AU2014264996B2 (en) 2017-08-24
WO2014180547A1 (de) 2014-11-13
RU2015150297A3 (ja) 2018-03-20
EP2994707A1 (de) 2016-03-16
CN105190211B (zh) 2018-07-03
UA118675C2 (uk) 2019-02-25
JP6383784B2 (ja) 2018-08-29
AU2014264996A1 (en) 2015-11-12
MX2015015320A (es) 2016-02-18
PL2994707T3 (pl) 2018-06-29
SI2994707T1 (en) 2018-06-29
AT514275A1 (de) 2014-11-15
AT514275B1 (de) 2015-05-15
CN105190211A (zh) 2015-12-23
US10215492B2 (en) 2019-02-26
ES2665143T3 (es) 2018-04-24
CA2910678C (en) 2021-12-21
BR112015027191B1 (pt) 2021-09-14
SG11201508937TA (en) 2015-12-30
CA2910678A1 (en) 2014-11-13
JP2016517949A (ja) 2016-06-20
US10914519B2 (en) 2021-02-09
BR112015027191A2 (pt) 2020-03-10
US20160061522A1 (en) 2016-03-03
US20190063836A1 (en) 2019-02-28
KR20160005751A (ko) 2016-01-15
MX366370B (es) 2019-07-05
MY175972A (en) 2020-07-19

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